一测多评法同时测定广西姜黄饮片中3种姜黄素类成分含量

目的：建立一测多评法同时测定广西姜黄饮片中双去甲氧基姜黄素、去甲氧基姜黄素、姜黄素含量，并验证方法准确性。方法：采用RP-HPLC进行含量测定，色谱柱为Shimadzu VP-ODS C₁₈柱（250 mm×4.6 mm，5 μm），流动相为乙腈-0.1%醋酸溶液（48：52），流速1.0 mL·min^-1，紫外检测波长为430 nm，柱温35 ℃，进样量20 μL。以姜黄素为参照物，建立其对双去甲氧基姜黄素、去甲氧基姜黄素的相对校正因子，计算后两者含量，经不同色谱系统和色谱柱间比较验证。同时运用外标法测定广西产区姜黄饮片中3个指标性成分的含量，比较计算值与实测值的的差异，以验证一测多评法的准确性和可行性。结果：双去甲氧基姜黄素、去甲氧基姜黄素、姜黄素进样量分别在0.032~0.80、0.042~1.05和0.105 6~2.64 μg范围内呈现良好线性关系；平均加样回收率（n=6）分别为98.81%、100.4%和100.3%，RSD分别为1.02%、1.32%和1.00%，该方法具有良好的重复性和耐用性；采用校正因子计算的含量值与外标法实测值之间无显著差异，结果各样品中总姜黄素含量依次为广西隆林野生（粗，3.65%）> 广西隆林栽培（中，3.47%）> 广西河池栽培（粗，3.01%）> 广西隆林野生（中，2.90%）> 广西隆林野生（细，2.72%）> 广西河池栽培（中，2.25%）> 广西河池栽培（细，2.12%）> 广西百色乐业栽培（中，1.75%）> 广西玉林北流栽培（中，1.44%）。结论：在对照品缺乏的情况下，利用相对校正因子可实现对姜黄饮片中双去甲氧基姜黄素、去甲氧基姜黄素含量测定，一测多评法可用于姜黄多种成分的质量评价。不同产地对广西姜黄质量有一定影响。

Objective: To establish a method for quantitative analysis of multi-components in Rhizoma Curcumae Longae by single-marker(QAMS),and validate its feasibility for quality evaluation. Methods: An HPLC method was applied for quality assessment using a Shimadzu VP-ODS C₁₈ column(4.6 mm×250 mm,5 μm). The mobile phase consisted of acetonitrile(solvent B)and 0.1% acetic acid water solution(solvent A) with fixed proportion(48∶52),and the flow rate was 1.0 mL·min^-1. The column temperature was set at 35 ℃. The chromatograms were monitored at 430 nm. The injection volume was 20 μL. Three main effective ingredients-bisdemethoxycurcumin,demethoxycurcumin,and curcumin,were selected as analytes to evaluate the quality of Rhizoma Curcumae Longae. The relative correction factors(RCFs)of curcumin to the other two ingredients were calculated. The method was evaluated by comparison of the quantitative results between external standard method and quantitative analysis of multi-components by single-marker(QAMS)method. Results: The peaks of bisdemethoxycurcumin,demethoxycurcumin and curcumin in the sample volume showed good linear relationship between 0.032-0.80 μg,0.042-1.05 μg and 0.105 6-2.64 μg. The average recoveries of them(n=6)were as follows:98.81%,100.4% and 100.3%,with the RSD as 1.02%,1.32%,and 1.00%,respectively.No significant differences were found in the quantitative results of three ingredients by neither external standard method nor quantitative analysis of multi-components(QAMS)method. The total contents of the above three curcumin ingredients in samples were as follows:wild from Longlin of Guangxi province(big,3.65%) >planting from Longlin of Guangxi province(middle,3.47%) >planting from Hechi of Guangxi province(big,3.01%) >wild from Longlin of Guangxi province(middle,2.90%) >wild from Longlin of Guangxi province(small,2.72%) >planting from Hechi of Guangxi province(middle,2.25%) >planting from Hechi of Guangxi province(small,2.12%) >planting from Leye of Guangxi province(middle,1.75%) >planting from Beiliu of Guangxi province(middle,1.44%). Conclusion: The established method is proved to be convenient and accurate in the determination of multi-components when some authentic standard substances were unavailable,and thus it can be used to control the quality of Rhizoma Curcumae Longae. Different origins in Guangxi province may have some effect on the quality of Rhizoma Curcumae Longae.